Process of producing carbon chlorids and silicon.



No. 745,637. PATENTED DEC. 1,1903.- F. J. MAOHALSKE. PROOESSOP PRODUCINGCARBON GHLORIDS AND SILICON.

APPLICATION FILED SEPT. 16, 1903.

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UNITED ii rrrss i atented December-.1, 1903.

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PROCESS OF PRODUCING CARBON CHLORIDSAND SILICON.

SIPECIFIGATION forming part of Letters Patent No. 745,637, datedDecember 1, 1903.

Application filed geptember 16, 1903.

To all whom it may concern.-

Be it known that I, FLORENTINE JOSEPH MACHALSKE, a citizen of the UnitedStates, residing at Brooklyn, in the county of Kings and State of NewYork, have invented certain new and useful Improvements in Processes ofProducing Carbon Ohlorids and Silicon, of which the following is aspecification.

According to this process a chlorid of silicon, usually thetetrachlorE-lfe c 'lsei. to react on a carbon compouhu, such as carbondisulfid or methane, under such conditions that the silicon and carboninterchange and the result-ing carbon chlorid is driven ofi, enabling it.to be condensed or utilized. The reaction is usuallyeffected in anelectric furnace and in an atmosphere which is non-oxidizing and freefrom water. When carbon disulfid is employed, the reaction between itand the silicon chlorid produces silicon sulfid, (SiS which may bereadily reduced to metallic silicon by heating it with carbon, theresulting carbon disulfid being again utilized in the first stage of theprocess. The silicon chlorid is preferably produced according to theprocess of my application, Serial No. 126,427, filed October 9, 1902, byheating a mixture of silica and sodium chlorid in an electricfurnace,from which the silicon chlorid is delivered as a gas.

A suitable apparatus for carrying out the process is shown in theaccompanying drawing, in which the figure if a vertical. angitudinalsection. It is to Lt, understood that this apparatus is merelyillustrative and that the process is in no way limited to its use.

The apparatus shown comprises an electric furnace A for the productionof the silicon chlorid, astructure B, havinga mixing-chamber whichreceives the silicon chlorid and carbon disulfid, with an electricfurnace for producing the disulfid, and an electric furnace O, whichreceives the mixed gases and. supplies the heat requisite to effect thereaction.

The furnace A comprises astack 1, of refractory non-conducting material,such as fire-brick, with a lining 2 of magnesia brick. Electrodes 8 3pass adjustably through refractory non conducting sleeves 4 in the sidesof the furnace. A charge-opening 5,

v with suitable closure, extends through the top Serial No. 173,456- (Nospecimens.)

wall. An outlet-flue 6 for the carbon chlorids rises from the upper endof the furnace and leads to the mixing-chamber. A tap-hole 7 leads fromthe lower part of the furnace withdrawnthrough the tap-hole 7. Aqueousvapor and air or other oxidizing atmosphere should be excluded from thefurnace during the operation. As it is undesirable that carbon' shouldbe present in the furnace in any form, the electrodes 3 are preferablyof metallic silicon. Silicon dichlorid may be produced instead of thetetrachlorid by emplaying a charge containing one part of silica and twoparts of sodium chlorid.

The structure B contains the mixing-chamber 9, which receives thesilicon chlorid from furnace A through the flue 6. Beneath themixing-chamber and opening into its lower end is an electric furnace 10,having electrodes 11, a charging-opening 12, and a taphole 13. Thisfurnace is used to produce carbon disulfid, a charge 14, which mayconsist of a mixture of carbon and sulfur, being placed around the endsof the electrodes and heated to the necessary temperature by an electriccurrent passed between them. The resulting vapors of carbon disulfidrise and escape through the passage 15 into the chamber 9, where theymix with the vapors of silicon chlorid from the furnace A. The gaseousmixture escapes from the chamber 9 through a fine 16 and is delivered tothe electric furnace O.

The furnace O serves to heat the mixed gases to the temperaturenecessary to effect the reaction between them. This furnace is ingeneral similar to the furnace A, one or more pairs 17 of electrodes,which may here be of carbon, platinum, &c., to heat the mixture ofsilicon chlorid and carbeing arranged.

bon disulfid by means of arcs sprung between the ends of the adjacentelectrodes. The carbon chlorid finally escapes through the outlet-flue18, andthe silicon sulfid also produced by the reaction may be withdrawnthrough the tap-hole 19. The silicon su fid from fu nace C may beconveniently en played for the production of carbon disulfid by chargingit, admixed with an equivalent amount of carbon, into the electricfurnace in lieu of or as an-addition to the charge of carbon and sulfur.The metallic silicon produced by the reduction of the i'silicon sulfidmay be withdrawn through the tap-hole 13. It is also obvious that carbondisulfid may be supplied from some outside source and that the vaporizeddisulfid and the silicon chlorid from the furnaceA may then be delivereddirectly into the reaction-furnace O.

Methane or.- other carbon compounds may be substitutedifor carbondisulfid as a source of carbon. When a mixture of one combining weightof silicon tetrachlorid and of methane is heatedyi to the propertemperature in the reaction-furnace (J, the silicon and carboninterchange with the production of carbon tetrachlorid and siliconhydrid, according-to the equation SiCl +OH =OOl +SiH This silicon hydridmay be ad antageousl used for the production of finelfi'i'1v1ued siliconcarbid or car-borundum by burning the hydrid in an atmosphereof carbondioxid. This reaction may be expressed by the following equation:

SiH +Oo =SiC+2H O.

I claim- I. The process of prod ucin g carbon chlorids, "which consistsin causing a substancecontaining carbon and a silicon chlorid to reactunder such conditions that the carbon is combined zvitltthe chlorin ofthe silicon chlorid, as set ort 2. The process of producing carbonchlorids, which consists in causinga carbon compound and a siliconchlorid to react under such conditions that the carbon compound isdecomposed and the carbon combined with the chlorin of the siliconchlorid, as set forth.

3. The process of producing,carb ou tetrachlorid, which consists incausing a carbon compound and silicon tetrachlorid to reac under suchconditions that thr cert-on compound is decomposed and the carbon comtosilicon by heating it in the tially non-oxidizing and free from water,to a temperature sufficient to cause the carbon to combine with thechlorin of the silicon chlorid, as set forth. a

6. The process of producing carbon chlorids, which consists in causingcarbon disulfid and a silicon chlorid to react with the production of acarbon chlorid and silicon sulfid, as set forth.

7.. The process'of producing carbon ch10- rids and silicon, whichconsists in causing carbon disulfid and a silicon chlorid to react withthe production of a carbon chlorid and silicon sulfid, and reducing saidsilicon sulfid presence of carbon, as set forth.

8. The process of producing silicon, which consists in heating siliconsulfid in the presence of a reducing agent, asset forth.

9. The process of producing carbon chlorids, which consists in heating amixture of silica and an alkali chlorid to a temperature sufficient toefiect the production of a silicon chlorid and an alkali oxid, mixingsaid silicon chlorid with a carbon compound, and supplying sufficientheat to cause the carbon compound to be decomposed and the carbon tocombine with the chlorin of the silicon chlorid, as set forth.

10. The process ofproducing carbon chlo-. ride, which consists inelectrically heating a mixture of substances containing carbon andsulfur, thereby producing gaseous carbon disulfid, mixing the carbondisulfid vapor with a silicon chlorid, and heating the mixture to atemperature sufficient to effert the production of the carbon chloridand silicon sulfid, as set forth.

In testimony whereof I have affixed m y signature in presence of twowitnesses.

FLORENTINE JOSEPH MAOIIALSKE.

Witnesses:

A. B. MARTIN, J AS. CANARY.

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